CN110940718B - Near-infrared photoelectric Ag2Preparation and test method of S @ Au cubic material - Google Patents

Near-infrared photoelectric Ag2Preparation and test method of S @ Au cubic material Download PDF

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CN110940718B
CN110940718B CN201911259719.6A CN201911259719A CN110940718B CN 110940718 B CN110940718 B CN 110940718B CN 201911259719 A CN201911259719 A CN 201911259719A CN 110940718 B CN110940718 B CN 110940718B
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陈晓梅
郑晨琰
郑敏莉
苏炳元
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XIAMEN CENTER FOR DISEASE CONTROL AND PREVENTION
Jimei University
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Abstract

The invention provides a near-infrared photoelectric Ag2The preparation method of the S @ Au cubic material comprises the following steps: placing the gold nanoparticle solution into a test tube, sequentially and respectively adding a formaldehyde solution and a Tollens reagent, mixing, and performing primary incubation at room temperature to obtain a first solution; when the color of the first solution changes from wine red to yellow, dropwise adding a sodium sulfide solution, and performing secondary incubation at room temperature to obtain a second solution; and centrifugally collecting the second solution, washing with ultrapure water, and dispersing in ultrapure water to obtain a target product Ag2S @ Au cubic material. And testing Ag by photoelectrochemical analysis2The near infrared photoelectric property of the S @ Au cubic material. The method has the advantages of simple synthesis steps, short time consumption and good photoelectric performance, and is particularly suitable for photoelectrochemical analysis application under the excitation of infrared light.

Description

Near-infrared photoelectric Ag2Preparation and test method of S @ Au cubic material
Technical Field
The invention relates to the technical field of inorganic semiconductor nano materials, in particular to near-infrared photoelectric Ag2A preparation method of an S @ Au cubic material.
Background
The Photoelectrochemical (PEC) analysis technique is a sensing technique that combines photochemistry and electrochemistry effectively, and an excitation source (light) and an output signal (electricity) are two completely different energy forms, so that the detection background signal is low and the sensitivity is high, and the technique has attracted much attention in the fields of biological analysis, food analysis, environmental analysis and the like. The photoelectrochemical sensing material is the core of the photoelectrochemical sensor, and the photoelectric property of the photoelectrochemical sensing material determines the analysis performance of the photoelectrochemical sensor.
At present, the methodMost PEC analyses employ visible/ultraviolet light as the light source to enable visible/ultraviolet light absorbing semiconductors (e.g., TiO)2ZnO and CdS) as the photosensitive material. Due to the limited penetration of visible/ultraviolet light, in the actual sample analysis, the sample needs to be pretreated in a more complicated way, which limits the practical application. Near Infrared (NIR) light refers to electromagnetic waves with wavelengths within the range of 780-2526nm, and compared with visible/ultraviolet light, NIR has strong penetrating power, can directly penetrate through tissues, glass and plastic packages for detection, and has great advantages in practical application. Nevertheless, in the field of photoelectrochemistry, only a few researchers have used NIR as a new light source for PEC sensing platforms, mainly due to the long wavelength and low energy of NIR, and it is difficult to find a photoelectric material that can efficiently absorb NIR and has a high PEC conversion activity. Therefore, the search for some new near-infrared photoelectric materials is beneficial to the development of advanced PEC sensing platforms.
Silver sulfide (Ag)2S) has unique photoelectrochemical properties, is a narrow-energy-band semiconductor material with high chemical stability, has a band gap of about 1.1eV, and has certain absorption capacity in a near infrared region. The gold nanoparticles have good conductivity and SPR effect, low toxicity and good biocompatibility, and can be widely applied to the field of sensing. Cubic nanoparticles have a larger contactable surface area than spherical nanoparticles, and are favored by various applications (e.g., drug therapy, analytical sensing) because of the abundance of atomic steps on the surface of cubic nanoparticles, which exhibit excellent photo/electro-catalytic properties. However, cubes are not as stable as spheres due to their structural anisotropy. This thermodynamic instability makes the formation of cubic crystals particularly difficult.
In the prior art, Li and the like are used for preparing Ag by a two-step method2S QDs/AuNPs composite material. Firstly, mixing silver nitrate, 3-mercaptopropionic acid and ethylene glycol, heating to 145 ℃, violently stirring for 25 minutes, and then centrifuging and collecting to obtain carboxyl-terminated Ag2S QDs solution. Then strengthening Ag by anchoring positively charged AuNPs2Photocurrent of S QDs. Long time consuming in the whole process, Ag2Synthesis of S QDsHigh-temperature reaction under the protection of argon is needed, and the cost is high.
Disclosure of Invention
Aiming at the problems of complex synthesis conditions, long time consumption, poor photoelectric property and the like of the existing infrared photoelectric material, the invention provides a near-infrared photoelectric Ag2The preparation and test method of the S @ Au cubic material solves the existing problems.
According to a first aspect of the present application, embodiments of the present application propose a near-infrared photoelectric Ag2The preparation method of the S @ Au cubic material comprises the following steps:
s1: placing the gold nanoparticle solution into a test tube, sequentially and respectively adding a formaldehyde solution and a Tollens reagent, mixing, and performing primary incubation at room temperature to obtain a first solution;
s2: when the color of the first solution changes from wine red to yellow, dropwise adding a sodium sulfide solution, and performing secondary incubation at room temperature to obtain a second solution; and
s3: centrifugally collecting the second solution, washing with ultrapure water, and dispersing in ultrapure water to obtain the target product Ag2S @ Au cubic material.
In some embodiments, the molar ratio of the formaldehyde solution to the Tollens reagent in step S1 is in the range of 5:4 to 5: 1. The Ag @ Au core-shell structure with a certain thickness can be prepared within the proportion range.
In some embodiments, the molar ratio of the sodium sulfide solution to the Tollens reagent ranges from 4:1 to 4: 4. In the proportion range, Ag with good near infrared photoelectric property can be prepared2S @ Au cubic material.
In some embodiments, the time for the first incubation is 10 minutes. The time of the first incubation can ensure that the Ag @ Au core-shell structure has a certain thickness.
In some embodiments, the second incubation time is in the range of 5-20 minutes. The time of the second incubation determines the Ag2And (3) completely preparing and molding the S @ Au cubic material.
In some embodiments, the target product obtained in step S3 is placed in a refrigerator and stored at a temperature of 4 ℃. The target product can be stored better at low temperatures.
According to a second aspect of the present application, embodiments of the present application propose a near-infrared photoelectric Ag2The test method of the S @ Au cubic material is characterized in that a target product is prepared by the preparation method of the first aspect, and the photoelectric property of the target product is tested by adopting a photoelectrochemical analysis method.
In some embodiments, the step of testing the photovoltaic properties of the target product comprises:
s4: cutting FTO glass, cleaning, drying, directly dripping a target product on the conductive surface of the FTO glass, and drying in an oven to obtain Ag2S@Au/FTO；
S5: mixing disodium hydrogen phosphate solution and sodium dihydrogen phosphate solution with different volume ratios to obtain phosphate buffer solutions with different pH values;
s6: constructing a photoelectrochemical measuring device by mixing Ag2S @ Au/FTO is used as a working electrode and is fixed by a platinum sheet electrode clamp, the reference electrode is an Ag/AgCl electrode, the auxiliary electrode is a platinum wire electrode, and the electrolytic cell is a transparent quartz electrolytic cell; and
s7: testing Ag in phosphate buffer solution by adopting a chronoamperometry and setting bias voltage to be 0V2Photoelectric behavior of S @ Au/FTO.
In some embodiments, the optoelectronic properties of the target product were tested using a 1W/cm infrared semiconductor laser as the light source. Using infrared light as light source to prove Ag2The S @ Au cubic material has certain infrared photoelectric property.
In some embodiments, the pH of the phosphate buffer solution in step S5 is in the range of 5 to 8. Phosphate buffers of different pH values have an influence on the measurement of the photoelectric properties.
The embodiment of the application discloses a near-infrared photoelectric Ag2The preparation and test method of the S @ Au cubic material adopts gold nanoparticles, Tollens reagent, formaldehyde and sodium sulfide as raw materials to synthesize Ag by a simple room temperature incubation method2The method is convenient, rapid and controllable, and the obtained Ag is2The S @ Au cubic material is goodGood near infrared photoelectric performance. Compared with other near-infrared photoelectric materials, the method has the advantages of simple synthesis steps, short time consumption and good photoelectric performance, and is beneficial to development of a novel PEC biosensing platform.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 shows a near-infrared photoelectric Ag film according to an embodiment of the present invention2The flow schematic diagram of the preparation method of the S @ Au cubic material;
FIG. 2 shows a near-infrared photoelectric Ag film according to an embodiment of the present invention2The flow schematic diagram of the testing method of the S @ Au cubic material;
FIG. 3 shows different contents of Tollens reagent vs. Ag in the first embodiment of the present invention2Influence of photoelectric properties of the S @ Au cubic material;
FIG. 4 shows different contents of sodium sulfide solution versus Ag for example two of the present invention2Influence of photoelectric properties of the S @ Au cubic material;
FIG. 5 is a graph of the different second incubation times versus Ag for example three of the present invention2Influence of photoelectric properties of the S @ Au cubic material;
FIG. 6 shows Ag in example four of the present invention2A photocurrent response diagram of the S @ Au cubic material;
FIG. 7 shows Ag in example four of the present invention2SEM image of S @ Au cubic material;
FIG. 8 shows Ag in example IV of the present invention2An EMI plot of S @ Au cubic material;
FIG. 9 shows Ag in example IV of the present invention2XRD pattern of S @ Au cubic material;
FIG. 10 shows pH vs. Ag in the PEC detection process of example five of the present invention2Influence of the photoelectric properties of the S @ Au cubic material.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the present invention will be described in further detail with reference to the accompanying drawings, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following examples, the preparation of gold nanoparticle solutions included the following steps:
in the first step, 5mL of chloroauric acid solution and 95mL of ultrapure water were mixed, heated and stirred until the solution was boiled.
In the second step, 10mL of trisodium citrate solution is added dropwise to the above mixed solution quickly, kept boiling and stirred continuously for 15 minutes, at which time the solution changes color from light yellow to wine red.
And thirdly, stopping heating, continuously stirring and cooling to room temperature to obtain a gold nanoparticle solution, and storing in a refrigerator at 4 ℃.
The preparation method of the Tollens reagent comprises the following steps:
in the first step, 1mL of 1% silver nitrate solution was added to the test tube after the test tube was washed with sodium hydroxide solution.
And secondly, adding 29mL of 2% dilute ammonia water dropwise while oscillating the test tube, then stirring until the precipitate completely disappears to obtain the target product Tollens reagent, and storing in a dark place.
The concentration of the Tollens reagent finally synthesized was 4X 10-3mol/L. The concentration of the trisodium citrate solution used in the examples was 38.8X 10-3mol/L, formaldehyde concentration of 0.01mol/L, sodium sulfide concentration of 1X 10-3mol/L。
As shown in FIG. 1, the embodiment of the present application proposes a near-infrared photoelectric Ag2The test method of the S @ Au cubic material comprises the following steps:
s1: placing the gold nanoparticle solution into a test tube, sequentially and respectively adding a formaldehyde solution and a Tollens reagent, mixing, and performing primary incubation at room temperature to obtain a first solution;
s2: when the color of the first solution changes from wine red to yellow, dropwise adding a sodium sulfide solution, and performing secondary incubation at room temperature to obtain a second solution; and
s3: centrifugally collecting the second solution, washing with ultrapure water, and dispersing in ultrapure water to obtain the target product Ag2S @ Au cubic material.
The target product is prepared by the preparation method of the first aspect, as shown in fig. 2, and another embodiment of the application provides a near-infrared photoelectric Ag2The test method of the S @ Au cubic material adopts a photoelectrochemical analysis method to test the photoelectric property of a target product, and specifically comprises the following steps:
s4: cutting FTO glass, cleaning, drying, directly dripping a target product on the conductive surface of the FTO glass, and drying in an oven to obtain Ag2S@Au/FTO；
S5: mixing disodium hydrogen phosphate solution and sodium dihydrogen phosphate solution with different volume ratios to obtain phosphate buffer solutions with different pH values;
s6: constructing a photoelectrochemical measuring device by mixing Ag2S @ Au/FTO is used as a working electrode and is fixed by a platinum sheet electrode clamp, the reference electrode is an Ag/AgCl electrode, the auxiliary electrode is a platinum wire electrode, and the electrolytic cell is a transparent quartz electrolytic cell; and
s7: testing Ag in phosphate buffer solution by adopting a chronoamperometry and setting bias voltage to be 0V2Photoelectric behavior of S @ Au/FTO.
The first embodiment is as follows:
in the first embodiment, a near-infrared photoelectric Ag is provided2The preparation method of the S @ Au cubic material comprises the following steps:
s1: putting 2mL of gold nanoparticle solution into a test tube, sequentially and respectively adding 0.5mL of formaldehyde solution and 1mL of Tollens reagent, 0.5mL of formaldehyde solution and 0.5mL of Tollens reagent, 0.5mL of formaldehyde solution and 0.25mL of Tollens reagent, mixing, and incubating for the first time at room temperature (25 ℃) for 10 minutes to obtain a first solution;
s2: when the color of the first solution changed from wine red to yellow, 1mL of sodium sulfide solution was added dropwise and a second incubation was performed at room temperature (25 ℃) for 10 minutes to obtain a second solution; and
s3: centrifugally collecting the second solution, washing with ultrapure water, and dispersing in ultrapure water to obtain the target product Ag2S @ Au cubic material, stored with the temperature set to 4 ℃ in a refrigerator.
The Ag synthesized under the condition that the formaldehyde solution and the Tollens reagent have different volume ratios is prepared by the steps2S @ Au, and the influence thereof on photocurrent response was measured, respectively, to obtain the results shown in FIG. 3, which illustrate that Ag prepared when 0.5mL of Tollens reagent was added, i.e., in the case where the volume ratio of the formaldehyde solution to the Tollens reagent was 1:1, i.e., in the case where the molar ratio of the formaldehyde solution to the Tollens reagent was 5:22The photocurrent intensity measured by the S @ Au cubic material is maximum.
Example two:
in the second embodiment, a near-infrared photoelectric Ag is provided2The preparation method of the S @ Au cubic material comprises the following steps:
s1: putting 2mL of gold nanoparticle solution into a test tube, sequentially and respectively adding 0.5mL of formaldehyde solution and 0.5mL of Tollens reagent, mixing, and incubating for the first time for 10 minutes at room temperature (25 ℃) to obtain a first solution;
s2: when the color of the first solution changes from wine red to yellow, 0.5mL, 1mL, 1.5mL and 2mL of sodium sulfide solution are respectively added dropwise, and a second incubation is carried out for 10 minutes at room temperature (25 ℃) to obtain a second solution; and
s3: centrifugally collecting the second solution, washing with ultrapure water, and dispersing in ultrapure water to obtain the target product Ag2S @ Au cubic material, stored with the temperature set to 4 ℃ in a refrigerator.
The Ag synthesized by adding sodium sulfide solution and Tollens reagent with different volume ratios is prepared by the steps2S @ Au, and their effects on photocurrent response were tested separately, yielding the results shown in figure 4, which illustrates that when 1mL of sodium sulfide solution was added,namely Ag prepared under the condition that the volume ratio of the sodium sulfide solution to the Tollens reagent is 2:1, namely under the condition that the molar ratio of the sodium sulfide solution to the Tollens reagent is 4:22The photocurrent intensity measured by the S @ Au cubic material is maximum.
Example three:
in the third embodiment, a near infrared photoelectric Ag is provided2The preparation method of the S @ Au cubic material comprises the following steps:
s1: putting 2mL of gold nanoparticle solution into a test tube, sequentially and respectively adding 0.5mL of formaldehyde solution and 0.5mL of Tollens reagent, mixing, and incubating for the first time for 10 minutes at room temperature (25 ℃) to obtain a first solution;
s2: when the color of the first solution changed from wine red to yellow, 1mL of sodium sulfide solution was added dropwise and a second incubation was performed at room temperature (25 ℃) for 5 minutes, 10 minutes, 15 minutes, and 20 minutes, respectively, to obtain a second solution; and
s3: centrifugally collecting the second solution, washing with ultrapure water, and dispersing in ultrapure water to obtain the target product Ag2S @ Au cubic material, stored with the temperature set to 4 ℃ in a refrigerator.
Preparing Ag synthesized under the condition of different secondary incubation times through the steps2S @ Au, and the influence of the S @ Au on the photocurrent response was respectively tested to obtain the results shown in FIG. 5, which illustrate that Ag prepared under the condition that the second incubation time is 10 minutes2The photocurrent intensity measured by the S @ Au cubic material is maximum.
Example four:
in the fourth embodiment, a near infrared photoelectric Ag is provided2The preparation method of the S @ Au cubic material comprises the following steps:
s1: putting 2mL of gold nanoparticle solution into a test tube, sequentially and respectively adding 0.5mL of formaldehyde solution and 0.5mL of Tollens reagent, mixing, and incubating for the first time for 10 minutes at room temperature (25 ℃) to obtain a first solution;
s2: when the color of the first solution changed from wine red to yellow, 1mL of sodium sulfide solution was added dropwise and a second incubation was performed at room temperature (25 ℃) for 10 minutes to obtain a second solution; and
s3: centrifugally collecting the second solution, washing with ultrapure water, and dispersing in ultrapure water to obtain the target product Ag2S @ Au cubic material, stored with the temperature set to 4 ℃ in a refrigerator.
The Ag is prepared by the steps2S @ Au, and the effect on photocurrent response was tested separately, yielding the results shown in fig. 6. As can be seen from the SEM image of fig. 7 and the EMI image of fig. 8: when the molar ratio of the formaldehyde solution to the Tollens reagent is 5:2, the molar ratio of the sodium sulfide solution to the Tollens reagent is 4:2, and the second incubation time is 10 minutes2S @ Au has a cubic structure, a particle diameter of about 1 mu m, and Ag as a core2S and Au are core-shell structures of the coating layers, and Ag can be seen from the XRD result in FIG. 92S and Au are present.
In summary, Ag was prepared when the molar ratio of formaldehyde solution to Tollens reagent was 5:2, the molar ratio of sodium sulfide solution to Tollens reagent was 4:2, and the second incubation time was 10 minutes2The S @ Au cubic material has the best infrared photoelectric property, a cubic structure and a core-shell structure.
Example five:
in example five, Ag was prepared by the method of example four2S @ Au cubic material and provides a near-infrared photoelectric Ag2The test method of the S @ Au cubic material comprises the following steps:
s4: cutting FTO glass into 1.5cm × 1.0cm (length × width), cleaning with acetone, ethanol and ultrapure water for 3 times, blowing with nitrogen, directly dripping the target product on the conductive surface of FTO glass, and drying in oven at 60 deg.C to obtain Ag2S@Au/FTO；
S5: different volume ratios of disodium hydrogen phosphate solution and sodium dihydrogen phosphate solution are mixed to obtain phosphate buffer solutions with different pH values. Specifically, 0.05mol/L disodium hydrogen phosphate solution and 0.05mol/L sodium dihydrogen phosphate solution are prepared and mixed to obtain a phosphate buffer solution, and the pH values of the phosphate buffer solution are respectively adjusted to 5, 6, 7.4 and 8;
s6: constructing a photoelectrochemical measuring device by mixing Ag2S @ Au/FTO is used as a working electrode and is fixed by a platinum sheet electrode clamp, the reference electrode is an Ag/AgCl electrode, the auxiliary electrode is a platinum wire electrode, and the electrolytic cell is a transparent quartz electrolytic cell; and
s7: at 1W cm-1An infrared semiconductor laser is used as a light source, a timing current method is adopted, bias voltage is set to be 0V, and Ag is tested in phosphate buffer2Photoelectric behavior of S @ Au/FTO.
Ag was prepared by the procedure of example four2The S @ Au cubic material is used for respectively testing the influence of phosphate buffers with different pH values on photocurrent response in a near-infrared response type photoelectrochemical measuring device, and the result shown in figure 10 is obtained. Ag obtained when the pH was 7.42The photoelectric property of S @ Au is optimal, and the photocurrent can reach 0.36 muA.
The embodiment of the application discloses a near-infrared photoelectric Ag2The preparation and test method of the S @ Au cubic material adopts gold nanoparticles, Tollens reagent, formaldehyde and sodium sulfide as raw materials to synthesize Ag by a simple room temperature incubation method2The method is convenient, rapid and controllable, and the obtained Ag is2The S @ Au cubic material has good near infrared photoelectric property. Compared with other near-infrared photoelectric materials, the method has the advantages of simple synthesis steps, short time consumption and good photoelectric performance, and is beneficial to development of a novel PEC biosensing platform.
It will be apparent to those skilled in the art that various modifications and variations can be made to the embodiments of the present invention without departing from the spirit and scope of the invention. In this way, if these modifications and changes are within the scope of the claims of the present invention and their equivalents, the present invention is also intended to cover these modifications and changes. The word "comprising" does not exclude the presence of other elements or steps than those listed in a claim. The mere fact that certain measures are recited in mutually different dependent claims does not indicate that a combination of these measures cannot be used to advantage. Any reference signs in the claims shall not be construed as limiting the scope.

Claims (7)

1. Near-infrared photoelectric Ag2The preparation method of the S @ Au cubic material is characterized by comprising the following steps of:
s1: placing the gold nanoparticle solution into a test tube, sequentially and respectively adding a formaldehyde solution and a Tollens reagent, mixing, and performing primary incubation at room temperature to obtain a first solution, wherein the molar ratio of the formaldehyde solution to the Tollens reagent is 5: 2;
s2: when the color of the first solution is changed from wine red to yellow, dropwise adding a sodium sulfide solution, and carrying out secondary incubation at room temperature to obtain a second solution, wherein the molar ratio of the sodium sulfide solution to the Tollens reagent is 4:2, and the time of the secondary incubation is 10 minutes; and
s3: centrifugally collecting the second solution, washing with ultrapure water, and dispersing in ultrapure water to obtain the target product Ag2S @ Au cubic material.
2. The near-infrared photovoltaic Ag of claim 12The preparation method of the S @ Au cubic material is characterized in that the first incubation time is 10 minutes.
3. The near-infrared photovoltaic Ag of claim 12The preparation method of the S @ Au cubic material is characterized in that the target product obtained in the step S3 is placed in a refrigerator and stored at the temperature of 4 ℃.
4. Near-infrared photoelectric Ag2A testing method of S @ Au cubic material, characterized in that the target product is prepared by the preparation method of any one of claims 1 to 3, and the photoelectric property of the target product is tested by a photoelectrochemical analysis method.
5. The near-infrared photovoltaic Ag of claim 42The test method of the S @ Au cubic material is characterized in that the step of testing the photoelectric property of the target product comprises the following steps:
s4: cutting, cleaning and drying the FTO glass, directly dripping the target product on the conductive surface of the FTO glass, and drying in an oven to obtain the Ag2S@Au/FTO；
S5: mixing disodium hydrogen phosphate solution and sodium dihydrogen phosphate solution with different volume ratios to obtain phosphate buffer solutions with different pH values;
s6: constructing a photoelectrochemical measuring device by mixing Ag2S @ Au/FTO is used as a working electrode and is fixed by a platinum sheet electrode clamp, the reference electrode is an Ag/AgCl electrode, the auxiliary electrode is a platinum wire electrode, and the electrolytic cell is a transparent quartz electrolytic cell; and
s7: testing Ag in phosphate buffer solution by adopting a chronoamperometry and setting bias voltage to be 0V2Photoelectric behavior of S @ Au/FTO.
6. The near-infrared photovoltaic Ag of claim 52The testing method of the S @ Au cubic material is characterized in that an infrared semiconductor laser with the wavelength of 1W/cm is used as a light source to test the photoelectric property of the target product.
7. The near-infrared photovoltaic Ag of claim 52The testing method of the S @ Au cubic material is characterized in that the pH value range of the phosphate buffer solution in the step S5 is 5-8.
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